CN109828012A - A kind of preparation method and application of the coplanar integrated interdigital electrode of three electrode - Google Patents
A kind of preparation method and application of the coplanar integrated interdigital electrode of three electrode Download PDFInfo
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- CN109828012A CN109828012A CN201910157594.XA CN201910157594A CN109828012A CN 109828012 A CN109828012 A CN 109828012A CN 201910157594 A CN201910157594 A CN 201910157594A CN 109828012 A CN109828012 A CN 109828012A
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Abstract
The present invention discloses the preparation method and application of the coplanar integrated interdigital electrode of three electrodes of one kind.Traditional three electrodes are concentrated into a plane of interdigital electrode by the present invention, are substantially reduced the size of three electrodes, convenient for the design and processing of microsensor, are particularly suitable for the sensor of Electrochemical Detection.In the coplanar integrated interdigital electrode of three electrode, working electrode is that yellow gold, silver, nickel, copper, cobalt or above-mentioned metal alloy layer is electroplated, it is platinum or carbon to electrode, reference electrode is silver chlorate, and working electrode and electrode distance is substantially reduced, the concentration polarization in solution can be eliminated, the intrinsic catalytic performance suitable for detecting electrode activated material.
Description
Technical field
The present invention relates to sensor technical fields, and in particular to the preparation side of the coplanar integrated interdigital electrode of three electrodes of one kind
Method and application.
Background technique
Biosensor technology is a kind of very active engineering technology, is to develop a kind of essential elder generation of biotechnology
Into detection and monitoring technology.Electrode is the most important sensitive components of electrochemical sensor.General sensor must have two
A above electrode, wherein three-electrode system is using relatively broad.Three electrodes include working electrode, reference electrode and to electrode.
Three electrodes of traditional three-electrode system are not in one plane integrated, between each electrode distance farther out, in electrification
Working electrode and to concentration polarization is easy to appear between electrode in test process is learned, measuring accuracy is influenced.In addition, traditional three electrodes
Size is big, is not easy to the design and processing of microsensor, limits the application of three-electrode system.
Interdigital electrode is common sensor sensing electrod assembly, is to have periodical figure in the face of such as finger-like or dressing
The electrode of case.Since interdigital electrode is a kind of micro- spaced electrodes structure, it is widely used in preparing microsensor.
Patent CN201710805378.2 discloses a kind of gas sensor that three electrodes are coplanar, in PET ganoine thin film base
Bottom surface uses screen printing technique machined electrode, and is sealed in electrode surface coating hydrophobic ventilated membrane.However, using silk
Net printing technology, the colloidal mixt generated in process can impact electrode detection sensitivity and stability.
Summary of the invention
For deficiency of the prior art, the present invention provides the preparation of the coplanar integrated interdigital electrode of three electrodes of one kind
Method and application, the interdigital electrode solve the problems, such as that three-electrode system can not be applied to microsensor, and obtained interdigital
Electrode is close due to working electrode and to distance between electrode, can eliminate the concentration polarization in Electrochemical Test Procedure significantly.
Substrate is used as using ceramics, silicon wafer, flexible material (such as PET, PI), high molecular material (FR-4 etc.), using electrochemistry film
Processing technology is electroplated, there is highly sensitive, high stable characteristic.
An object of the present invention be to provide a kind of working electrode, reference electrode with to the coplanar integrated height of three electrode of electrode
Accurate interdigital electrode.
Further, the interdigital electrode is ceramics, silicon wafer or high molecular polymer base interdigital electrode.
Further, the ceramics are aluminium oxide or aluminium nitride.
Further, the working electrode of the interdigital electrode is that yellow gold, silver, nickel, copper, cobalt or above-mentioned metal alloy is electroplated
Layer, it is interdigital in one refer to be reference electrode, it is another to refer to as to electrode.
The second object of the present invention is to provide the preparation method of the coplanar integrated interdigital electrode of three electrodes of one kind, including it is as follows
Step:
(1) ceramic matrix, silicon wafer or high molecular polymer substrate are subjected to laser boring.
(2) substrate after punching is realized in surface metalation, including hole by magnetron sputtering and is metallized.
(3) whole plate substrate copper facing is formed into copper electroplating layer.
(4) by the substrate for having plated copper, plating metal forms electroplated metal layer again.
(5) it is coated with photoresist, interdigital electrode is exposed on litho machine, it is then profiling, form interdigital electrode pattern.
(6) etching forms route, then photoresist is removed in potassium hydroxide solution, forms working electrode.
(7) wherein one referring to that electroplatinizing or carbon are used as to electrode for interdigital, silver chlorate is electroplated as reference electrode in another finger,
To form the coplanar interdigital electrode of three electrodes.
Further, the metal of the metal layer is yellow gold, silver, nickel, copper, cobalt or above-mentioned metal alloy.
Further, the copper electroplating layer can be replaced with silver layer or layer gold.
Further, step (2) by magnetron sputtering formed sputtering layer, every layer of sputtering layer with a thickness of
Further, the copper electroplating layer with a thickness of 2 μm.
Further, it is described plating layer gold with a thickness of 1 μm.
The third object of the present invention is to provide the application of interdigital electrode of the invention, it is characterised in that is total to three electrode
The integrated interdigital electrode in face is for the relevant biology of electrochemistry and electro-chemical activity detection.
Further, the interdigital electrode pattern precision after present invention processing in the micron-scale, using semiconductor machining, is suitable for
The use of MEMS and miniature electrochemical device.
Further, interdigital electrode of the invention is applicable to the electrification of the intrinsic catalytic performance of detecting electrode active material
Learn device.
The beneficial effects of the present invention are:
(1) traditional three electrodes can substantially be narrowed down under several millimeters of size, is processed convenient for the design of microsensor,
In particular for the sensor of Electrochemical Detection.
(2) working electrode and electrode distance is substantially reduced, working electrode and to electrode distance between 50-100 μm, can
The concentration polarization in solution is eliminated, can detect the intrinsic catalytic performance of electrode activation material.
(3) semiconductor technology is used, pure metal is electroplated in electrode surface, greatly improves the sensitivity and stabilization of electrode
Property, it can be used for high-accuracy detection environment.
Detailed description of the invention
Fig. 1 is three electrodes interdigital electrode produced by the present invention.
Fig. 2 is interdigital electrode the two poles of the earth NPG electrode (left side) made from embodiment 1, Pt/Au electrode (right side).
Fig. 3 is platinum electrode made from embodiment 2.
Fig. 4 is the coplanar integrated interdigital electrode (TEIE electrode) of three electrodes of the preparation of embodiment 1 in 0.1MKOH+5mM grape
Test obtains electrochemical impedance spectroscopy (EIS) (a) and equivalent circuit diagram (b) in sugar+0.01MKCl solution
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1:
The coplanar interdigital electrode of three electrodes is processed on aluminium oxide ceramic substrate
(1) it is directed to the aluminium oxide of 0.38mm thickness, laser boring forms the laser hole of 100 μ m diameters.Whole plate magnetron sputtering, shape
At titanium-tungsten layer and albata layer, wherein titanium-tungsten ratio is 70%:30%, and corronil ratio is 70%:30%,
Two layers of thickness is
(2) 2 μm of electro-coppering, in copper sulphate 50g/L, sulfuric acid 100g/L, copper facing in potassium chloride 20ppm, PSP20ppm solution,
Current density is 1.5ASD.
(3) nano-porous gold is plated using method documented by patent application CN108802140A, Gold plated Layer is 1 μm.
(4) it is coated with photoetching development.
(5) etching is formed on this basis, and etching solution is hydrofluoric acid and nitric acid, and molar ratio 3:1 forms gold line
Road, the hot travel route are working electrode.
(6) photoresist is removed in the potassium hydroxide solution of 10mol/L, is formed for one of electrode plating platinum to electricity
Pole, electroplating solution are nitric acid 2g/L, sulfuric acid 10g/L, potassium sulfate 20g/L, citric acid 30g/L, H2PtCl61mM, KCl20g/L, pH
It is 5.0, current density 1.0ASD.Plating silver chlorate forms reference electrode on the other electrode, first in the nitric acid of 5mol/L
Electrode is applied anode current by electrosilvering in silver-colored solution, and plating forms silver chlorate in the Klorvess Liquid of 2M.
Embodiment 2:
Three-electrode system is formed on polyphosphazene polymer imide membrane surface
(1) laser boring, then magnetron sputtering, SiO2/ Ti/Cu, layer gold with a thickness of
(2) 2 μm of electro-coppering, in copper sulphate 50g/L, sulfuric acid 100g/L, copper facing in potassium chloride 20g/L, PSP20ppm solution,
Current density is 1.0ASD.
(3) gold-plated, Gold plated Layer is 1 μm.
(4) it is coated with photoetching development.
(5) etching is formed on this basis, and etching solution is hydrofluoric acid and nitric acid, and molar ratio 3:1 forms gold line
Road.
(6) photoresist is removed in the potassium hydroxide solution of 10mol/L, for one of electrode plating platinum, be electroplated molten
Liquid is nitric acid 2g/L, sulfuric acid 10g/L, potassium sulfate 20g/L, citric acid 30g/L, H2PtCl61mM, KCl20g/L, pH 5.0, electricity
Current density is 1.0ASD.Silver chlorate is electroplated on reference electrode, first the electrosilvering in the silver nitrate solution of 5M, electrode is applied into sun
Electrode current, plating forms silver chlorate in the Klorvess Liquid of 2M.
Embodiment 3:
On borate glass surface, processing is used for the catalytic activity of photoelectric coupling detecting electrode catalysis material
(1) laser boring on silica surface, then magnetron sputtering, SiO2/ Ti/Cu, layer gold is with a thickness of 100nm.
(2) 2 μm of electro-coppering, in copper sulphate 50g/L, sulfuric acid 100g/L, copper facing in potassium chloride 20g/L, PSP20ppm solution,
Current density is 1.5ASD.
(3) gold-plated, Gold plated Layer is 1 μm.
(4) it is coated with photoetching development.
(5) etching is formed on this basis, and etching solution is hydrofluoric acid and nitric acid, and molar ratio 3:1 forms gold line
Road.
(6) photoresist is removed in the potassium hydroxide solution of 10mol/L, for one of electrode plating platinum, be electroplated molten
Liquid is nitric acid 2g/L, sulfuric acid 10g/L, potassium sulfate 20g/L, citric acid 30g/L, H2PtCl61mM, KCl0.1mM, pH 5.0, electricity
Current density is 1.0ASD.Silver chlorate is electroplated on reference electrode, first the electrosilvering in the silver nitrate solution of 5mol/L, electrode is applied
Add anode current, plating forms silver chlorate in the Klorvess Liquid of 2mol/L.
Application examples
The coplanar integrated interdigital electrode (TEIE electrode) of three electrodes prepared by embodiment 1 0.1MKOH+5mM glucose+
Test obtains electrochemical impedance spectroscopy (EIS) and single NPG electrode Fig. 4 (a) as a control test in 0.01MKCl solution, and
Equivalent circuit diagram Fig. 4 (b).
All there are two half circuits for TEIE electrode and NPG electrode, it means that their transmission characteristic is similar.It can from Fig. 4
To find out, the equivalent series resistance (Rs) of TEIE electrode (2.362 Ω) is much smaller than NPG electrode (16.930 Ω), shows by making
With this novel three-electrode structure of the present invention, sheet resistance and bulk resistor can be significantly reduced.In addition, TEIE electrode has
The charge transfer resistance (Rct) of 1.516 Ω is much smaller than NPG electrode (90.780 Ω), represents the electric charge transfer speed of TEIE electrode
Quickly.
In view of polarization process, using constant phase element (CPE or Q).CPE is determined by two parameters CPE-T and CPE-P
Justice.In general, the element is controlled by diffusion process (Warburg impedance) when CPE-P is 0.5.If CPE-P is 1 or 0, divide
Desired electrical perhaps pure resistance is not represented.The CPE-P value of TEIE electrode and NPG electrode is fitted to 0.9018 and 0.5493.It can see
Out, NPG polarization of electrode process is spread closer to Warburg, and interdigital electrode is more relevant with capacitance behavior.
It can also be seen that TEIE electrode has the polarization resistance (Rp) of 62.000 Ω, less than the Rp of NPG electrode from Fig. 4
(100.600Ω)。
From this application examples can be seen that working electrode in TEIE electrode and to the interval between electrode it is small, can effectively delay
Concentration polarization is solved, better electric charge transfer and polarization process are conducive to.
Claims (10)
1. a kind of coplanar interdigital electrode of three electrodes, it is characterised in that: working electrode, reference electrode and to the coplanar integrated fork of electrode
Refer to electrode, wherein working electrode in interdigital electrode is that yellow gold, silver, nickel, copper, cobalt or above-mentioned metal alloy layer is electroplated, it is interdigital in
One refer to be reference electrode, it is another to refer to as to electrode.
2. a kind of coplanar interdigital electrode of three electrode according to claim 1, it is characterised in that: the interdigital electrode is pottery
Porcelain, silicon wafer or high molecular polymer base interdigital electrode.
3. a kind of coplanar interdigital electrode of three electrode according to claim 2, it is characterised in that: the ceramics be aluminium oxide or
Aluminium nitride.
4. a kind of coplanar interdigital electrode of three electrode according to claim 1, it is characterised in that: described to electrode platinum plating or plating
Carbon, reference electrode plate silver chlorate.
5. a kind of coplanar interdigital electrode of three electrode according to claim 1, it is characterised in that: working electrode and to electrode spacing
From between 50-100 μm.
6. a kind of preparation method of the coplanar interdigital electrode of three electrode according to claim 1, which is characterized in that including as follows
Step:
(1) ceramic matrix, silicon wafer or high molecular polymer substrate are subjected to laser boring；
(2) substrate after punching is realized in surface metalation, including hole by magnetron sputtering and is metallized；
(3) whole plate substrate copper facing is formed into copper electroplating layer；
(4) by the substrate for having plated copper, plating metal forms electroplated metal layer again；
(5) it is coated with photoresist, interdigital electrode is exposed on litho machine, it is then profiling, form interdigital electrode pattern；
(6) etching forms route, then photoresist is removed in potassium hydroxide solution, forms working electrode；
(7) using interdigital a wherein finger electroplatinizing or carbon as to electrode, silver chlorate is electroplated as reference electrode in another finger, thus
Form the coplanar interdigital electrode of three electrodes；
Metal in the metal layer is yellow gold, silver, nickel, copper, cobalt or above-mentioned metal alloy.
7. preparation method according to claim 6, it is characterised in that: the copper electroplating layer silver layer or layer gold replace.
8. preparation method according to claim 6, it is characterised in that: the step (2) is formed by magnetron sputtering and sputtered
Layer, every layer of sputtering layer with a thickness of
9. a kind of sensor comprising the coplanar interdigital electrode of three electrodes described in claim 1 or preparation as claimed in claim 6
The coplanar interdigital electrode of three electrodes made from method.
10. a kind of gas detection equipment, it is characterised in that: include sensor as claimed in claim 9, and connect with sensor
The control module connect, the output module being connect with control module.
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| CN110320256A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for measuring micro lead in water |
| CN110333276A (en) * | 2019-06-28 | 2019-10-15 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for fast detection of trace cadmium |
| CN110455899A (en) * | 2019-07-16 | 2019-11-15 | 广州钰芯传感科技有限公司 | A kind of electrochemical gas sensor and its device packaging method |
| CN110530944A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | It is a kind of based on the portable minisize glucose of copper-based nano composite construction without enzyme sensing electrode and the preparation method and application thereof |
| CN110530952A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | A kind of card insert type electrochemical gas sensor mould group and its packaging method |
| CN110530943A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | A kind of flexible enzyme-free glucose sensing electrode and preparation method thereof of rear-earth-doped cobalt phosphorus ternary alloy three-partalloy modification nano porous copper |
| CN110554073A (en) * | 2019-07-23 | 2019-12-10 | 广州钰芯传感科技有限公司 | Magnetic attraction type packaged electrochemical gas sensor and packaging method thereof |
| CN111879827A (en) * | 2020-06-15 | 2020-11-03 | 上海集成电路研发中心有限公司 | Flexible sensor structure and preparation method thereof |
| CN112117131A (en) * | 2019-06-21 | 2020-12-22 | 清华大学 | Interdigital electrode based on three-dimensional nano porous gold and preparation method and application thereof |
| CN113702477A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Gold film modified electrode for heavy metal detection and preparation method thereof |
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| CN112117131A (en) * | 2019-06-21 | 2020-12-22 | 清华大学 | Interdigital electrode based on three-dimensional nano porous gold and preparation method and application thereof |
| CN110320256A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for measuring micro lead in water |
| CN110333276A (en) * | 2019-06-28 | 2019-10-15 | 广州钰芯传感科技有限公司 | A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for fast detection of trace cadmium |
| CN110455899A (en) * | 2019-07-16 | 2019-11-15 | 广州钰芯传感科技有限公司 | A kind of electrochemical gas sensor and its device packaging method |
| CN110554073A (en) * | 2019-07-23 | 2019-12-10 | 广州钰芯传感科技有限公司 | Magnetic attraction type packaged electrochemical gas sensor and packaging method thereof |
| CN110530944A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | It is a kind of based on the portable minisize glucose of copper-based nano composite construction without enzyme sensing electrode and the preparation method and application thereof |
| CN110530952A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | A kind of card insert type electrochemical gas sensor mould group and its packaging method |
| CN110530943A (en) * | 2019-08-19 | 2019-12-03 | 广州钰芯传感科技有限公司 | A kind of flexible enzyme-free glucose sensing electrode and preparation method thereof of rear-earth-doped cobalt phosphorus ternary alloy three-partalloy modification nano porous copper |
| CN110530952B (en) * | 2019-08-19 | 2022-05-17 | 广州钰芯传感科技有限公司 | Card-inserting type electrochemical gas sensor module and packaging method thereof |
| CN110530943B (en) * | 2019-08-19 | 2022-07-12 | 广州钰芯传感科技有限公司 | Flexible enzyme-free glucose sensing electrode and preparation method thereof |
| CN111879827A (en) * | 2020-06-15 | 2020-11-03 | 上海集成电路研发中心有限公司 | Flexible sensor structure and preparation method thereof |
| CN113702477A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Gold film modified electrode for heavy metal detection and preparation method thereof |
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Application publication date: 20190531 |